Countercurrent hydrolysis of fat



4 M. H. ITTNER CCUNTERCURRENT HYDROLYSIS OF FAT Filed Oct. 27, 1944 IN I vE NTo MM BY a; ,6 7% f ATTQEZEY Patented Aug. 30, 194 *2 COUNTERCURRENT HY DROLYSIS F FAT Martin Hill Ittner, Jersey City, N. J., assignor to Colgate-Palmolive-Peet Company, Jersey City, N. J., a corporation of Delaware Continuation of application Serial No. 240,037, November 12, 1938, which is a division of application Serial No. 83,991, June 6, 1936. This application October 27, 1944, Serial No. 560,641

This invention relates to improved apparatus for the aqueous saponification or hydrolysis of fats and'fatty oils to produce fatty acids and glycerine.

Fats and fatty oils as they occur in nature con- 5 value for the commercial hydrolysis of fats and sist of triglycerides, that is, compounds in which fatty oils to produce fatty acids and glycerine. one molecule of glycerine has been combined It has also been proposed to accomplish the with three molecules of fatty acid with the elimaqueous hydrolysisof fats and fatty oils by heatination of three molecules of water. It is the ing the fats or fatty oils together with liquid object of this invention to provide an improved 1 Water at comparatively. high temperatures, and apparatus for splitting or hydrolyzing such triat pressures sufficient to preventthe formation of glycerides into fatty acids and glycerine, with steam in contact with the mixture being heated, the production of a relatively concentrated aqueh t pro u t o o n q eous solution of ous solution of 'glycerine and relatively pure fatty yc rine and the fatty acid. 7 acids uncontaminated by decomposition prod- In l such procedures which have been used ucts or tars or by catalytic materials or reaction or pr p s d r r an d a t ns, wh h products ofcatalytic materials. so to an equilibrium, result, and the saponifica- The saponification of fats and oils with caustic i n or hydrolysis. as the Case y is incomalkali in excess, or in-the proper proportions to Plate, pt W repetitions of the treatmentcombine th t fatty acids produced, has long Except under very favorable conditions, the been used in the manufacture of soap. Glycerine saponificetion o drolys s seldom proceeds as is produced at thesame time that the soap is far as completion" By removing the aq produced, but the removal and purification of the ous solution of glyce ne formed and subjectin glycerjne involves number of'relativel expen; the fatty matter to repetitions of the treatment, give operations a the saponification or hydrolysis may be brought The aqueous hydrolysis of fats and fatty oils, up to 95% of completion, or, under favorable by the use of water and catalysts'of various types wndltions, s h higher- Furthermore, has also been known and used for a long time. t on and-protracted treatment are required Included among the catalysts Which'have been to o complete the reaction, and t e heat losses used are lime, magnesia, and other basic which take place because of the repetition of the terials, and sulphuric acid and other acids. treatment and the h-of the treatment be- Aqueous hydrolysis with the aid of such catalysts come excessive- If Water is n t used freely in has generally been carried out in an autoclave carrying o the leactiontthe p fi ation Or in the presence of liquid water and steam under yt y s retarded; and if Water is used freely, moderate pressure, such as pressures from 120 If many changes ofwater are used, the lycto 150 pounds. per square inch while employing Brill? Obtained s' j a y d l ted, and exagitation from jet steam or mechanical stirrer Denslve 130 evaporate and concentrate- A180, to promote surface contact between fat and Where the treatment is Prolonged p ated, water. there is an increase in the darkening of the fatty Another method of accomplishing the aqueous o acids and the formation of undesirable tars. hydrolysis of fats and fatty oils is the well known This is P c a y rue inthe processes in which Twitchell process in which the fat or fatty oil is C talysts are used. i brought into contact with water and one of the Where catalysts are used to hasten the saponiso-called Twitchell reagents, which are acid catafication or hydrolysis, the products produced are lysts which possess the property of emulsifying contaminated by the catalysts and special treatthe fat or fatty oil and of dissolving to some ment is required to remove the catalysts; extent in the fat or fatty oil, at the boiling point As an illustration of the fact that these hyof water. drolyses or saponifications as commonly carried It is also-well known that fats and fatty oils out are balanced or reversible reactions which do hydrolyze to some extent when in contact with not go to completion even at high-temperatures wateralone at relatively low temperatures, e. g.,

4 Claims. (Cl. 260-415) temperatures up to about the-boiling point of water. This hydrolysis, while sufiiciently fast to cause fats and fatty oilsstored in the presence of moisture to deteriorate, is too slow to be of and pressures, I have determined that if a mix- 3 ture containing 35 parts of pure neutral tallow and 25 parts of pure water is heated under pressure in an autoclave to about 255 C. for about 3 hours, or until an equilibrium is reached, a product is obtained which is about 92% hydrolyzed. If a mixture containing glycerine and pure tallow fatty acids, in the exact amounts which would be obtained by complete hydrolysis of 35 parts of pure neutrahtallow. and. sufficient watento make the total 'GQ parts is heated in an autoclave to 255 C. for 3 hours and at the same pressure as employed in the test described above, an esterification takes place with the formation of glycerides and with the production of l a mixture about 92% hydrolyzed. Thus. the. same equilibrium is arrived at whetherneutral. tall ow and water are heated together, or whether tallow fatty acids, glycerine and water are heated together. Similar experiments with coconut oil indicate that the same phengmenon occurs except that a larger proportio n oi wateris required for the same degree of hydrolysis. At lower 'temperatures and pressures, longer periods. are 126-.- quired for the reactiorgto reach an equilibrium o nt. d. t; autumn) e; yd oly is: smisiderably less l ac -f let ceeds to an.eq

1%- mu t n-. 5 3 19? P ri lletana i 9 93 91 1 1 is in accordancew ith the well V hl wn ewmas action. Eurtherfore, as well known the use of catalysts in speedi causes h l tal c ch h s; quili iu in irie weeriqm ime By emes? 9 i9. -.R ':9 V. a ara u for hes lbslan nip eta uequ h o y of fatsand fatty o ils ma single; operationand within a relatively shor tirneand with. marked heat economy, with thaproduction of relatively concentratedaqueous:

, ely li ne. a tty. ac ds c amlnets ih a ata ys s-.01 ther, b e ti ne. p rit es. equi in pecial: r atm n for i .v emq ll f nd withqufit he bj t ona l c: e os tionand o mati n t er er to o e requently n i lntexed whee ar r ne he d o i even o a lesse exte tit authatltocwhich Icarry it.

ha ound; hat. althou h the olubility. of water in f ats and fa tty acids iswery slight at low temperatures, and-at temperatures as high as the il n point water.

at. atmospheric pressure or ven mn iderah r lehenhe s lu ili y .of. water in fat and fatt l il .ahd-z a tylacidsin the pr s-. ence. c ss;water ..uncl r. llfilci nt pressure. to ent; hez mr at enei he water, incr ases slowly uptqabo t 0 q: and then. increases mo e ld y-atrh her emperatur s- In al ca e to dissolve any considerable; amountofvwater in the fats or. fatty acids apressure in excess .of .the pressure of saturated watervapor at. the temperature selected:mustbe used. For example. at atemperaturegofu235fi Q. andan absolute pressure of roundsperi quara nch. atty ac ds from coconut oil will dissolve aboutj] .of their weight of a e n; he. reseneea f. exces l quid wa er- The same fatty acids, in the presence. of excess liquid water, andata temperatureof 25 C. and an absolute..pr essure .of. =-8Qfl .,p.o unds. per square inch dissolve .about- 20%;.of..waten; At a. tempera.- ture of about28fZ crandapressure in excesspf'lo h slt es i tt c ds-blendfreely with e. an,-.th. ir. own .weightoi. water, with the formation of. ;a single,- clear liquidphase. Other commercial fatty. acids,.suclr as .thosefrom tallovv and ,palm oil behaye.- in= assimilanmanner and lllredzf have an increased power to dissolve water at elevated temperatures and pressures such as those above referred to.

In using the apparatus of the present invention, I subject the fat, fatty oil, or mixtures thereof to be hydrolyzed to the action of liquid Water at high temperatures and pressures. The process is carried out by contacting the fatty material with. the waten bycountercurrent flow under such conditions as; to insure intimate contact of the fatty material with the water, with prevention or minimizing of emulsification, and with the use of temperatures and pressures sufiiciently hightoinsure that an amount of water appreciablyin excess of the amount of water the c ornplete hydrolysis of the fatty material tp fat ty acids and glyc'erine is dissolved in the fatty material but not so high as to produoemiscibility of. the fatty material and water, or tocausethe fatty material to dissolve all of the water used with the production of a single The amount of water required to be dissolved in the fatty material varies with different fatty materials, but in each case, for the rapid hydrolysis. of; thepresent invention, must beapreciably,-greater.- thantha amount required for hydrolysis. FOX-EXflIIlRlfiyfiOCOIlllfi oil for complete hydrolysis requires about 8.3 of its own weight of water? and tallow requires, about 6. 1% of'itsownweight of water. For this rapid hydrolysis of these; fatsi the; effective conditions of temperature andpressureare such that the fatty material dissolves: considerably. more water than these-amounts Thewaten dissolved in the fat affects the sap onification and-any excess water not dissolved washes, out g-l cerine so, v that the r ficationmay. hus e: ar d comp o The totalamount of waterused must be sufilclent n onl ;--nro d e: n s ary amount liquid phase.

of water for the hydrolysis ,1 and any excesswater dissolved in the fattyr material-at the high tem-. peratures and; pressure;employed but,also sufficient to d issolve;the glycerine formedandremove it from the fatty-material an aqueous solution. When using theapparatus l can ,obtainglycerine in aqueous; solutions of;concentrations ranging from 15% or;less-.to;50%- or sornewhat more, diect v. and h i mo ntmi: rs s i r ying out my process should be such as-to give a slvc e solu on-1 eides red;co cen ion:

In v carrying out thisprocess with; countercurrent flow oi the fatty rnaterial to,be saponified 't ter. th ressur lmai ta uedz n-t an: paratus is wellin excess of -the. pre ss ure ;of satu-, rated steam; at;the highest: temperature selected, so h ord nary a iat Qns-in: empe a e and r su e t nnqts sultinthev p rl t o of wa r th t e pparetuszto t rf re with-t e operation of the ro e s; Thelapparatusiszkept completely full of, liquid,, that is; fatty-material and a eousge rc rinel.

It is important; inazcarryinggoutthelprocess, to provide for the proper separation of the aqueous glycerine; froml the. 7 fatty material, at the point Where the, aqueousglycerina is tremoved from the apparatus, andto pr,o,vide.- for the; proper; separation of, the-fattyl-lmaterials that -is,. the fatty acids resulting; from; the; hydrolysis, from the Water at the point where the fatty-.acids are withdrawn from the apparatus; Thisis accomplished by p foviding settling. spaces .orozones adjacent to the parts of the apparatus at which thesematerials. are-.removed, so. that where the =-aque0us glycerine is.separated on---removed=from the-apparatus, there; provided a quiescent zone in which the aqueous glycerine may separate from the fatty material to permit the removal of aqueous glycerine free from fatty material except in so far as the fatty material may be dissolved in the aqueous glycerine; otherwise, the incoming fatty material will readily emulsify with and be largely removed by the outwardly flowing current of aqueous glycerine when the equipment is being used at an economic rate of operation as the fatty material is very prone to objectionable emulsification in its early stages of hydrolysis. Similarly, at the point where the fatty acids are removed from the apparatus, there is provided a quiescent zone where the fatty acids may separate from the water, and be removed without removing water at the same time, except in so far as the water may be'dissolved in the fatty material. Because of the fact that the temperatures and pressures are sufiiciently high in my process to cause a very considerable amount of water to actually dissolve in the fatty matter, agitation is not needed to promote saponification but leads to emulsification that is generally considered as desirable, if not necessary, to increase contact in other methods employing temperatures and pressures not suificiently high to cause a considerable degree of solubility of water in the fatty material. Emulsification in any part of the apparatus lessens the eiilciency of the process and emulsification of inflowing fat with aqueous glycerine or of outflowing fatty acids with inflowing water besides disturbing the smooth operation of the process also introduces an indefinite and irregular factor in the proportions of reacting materials remaining in the apparatus.

While the process can be carried out over a fairly wide range of temperatures, which varies with different fatty materials, and over a fairly wide range of pressures, which more or less depends upon the temperatures selected, the temperatures used, and the corresponding pressures used, must be such that two separate and distinct liquid phases are maintained within the apparatus, one phase being the fatty material, that is, the fat or fatty oil, or the fatty acids, or partially hydrolyzed fatty material, containing a proportion of dissolved water somewhat greater than the amount of water required for the complete hydrolysis of the fatty material, and the other phase consisting of water or aqueous glycerine, sumcient in amount to effectively wash out the glycerine from the fatty material and carry it through the apparatus, to be removed as aqueous glycerine ranging in concentrations from 15% or less up to 50% or more. Stirring or emulsification defeats the washing by preventing the ready separation of the aqueous glycerine phase from the fatty phase and efficient washing out of glycerine. The pressure selected depends upon the temperature and must be sufficient to maintain the material in a liquid state with no vaporization, and should be considerably in excess of the pressure of saturated steam at the temperature selected, to prevent vaporization of water if a slight drop in pressure or increase in temperature takes place, and to favor solution of water in the fatty material.

While no definite temperature limits can be given for carrying out the process, inasmuch as the temperatures vary with different fats or fatty oils, I have found that coconut oil, for example, can be advantageously treated at temperatures of around 235 C. or 245 C. and at pressures ranging about 250 pounds, more or less, in excess of the pressure of saturated steam at these tem-'* peratures, and that other fats and fatty oils may be advantageously treated at similar temperatures and approximately similar excess pressures. At temperatures of about 287 C. or higher and correspondingly high pressures, I find that the process cannot be carried out with coconut oil, as at these high temperatures and pressures coconut oil fatty acids blend freely with more than their own weight of water to form a single clear liquid phase, instead of the two phases required for the proper operation of my process. Similarly, with each fat or fatty oil, there is an upper temperature limit beyond which the solubility of the water in the fatty material is too great to permit the process to be carried out.

In general, I find that temperatures somewhat above about 200 (2., or a little below 200 C., are satisfactory, in that at such temperatures the solubility of the water in the fatty material is quite appreciable and is in excess of the amount required for the hydrolysis of the fat or fatty oil, but is not so great as to cause the formation of a single liquid phase in the apparatus or to render the water so soluble in the fatty material as to preclude the proper washin out of the glycerine, at least with a reasonable amount of water. At lower temperatures, Water is not sufficiently soluble in the fatty material to allow the process to be economically carried out, and the desired hydrolysis cannot be obtained at such lower temperatures in apparatus which does not depend upon mixing and large surface contact, at least in a reasonably short time and with the production of concentrated aqueous glycerine sub stantially free from fatty material.

In the apparatus of the invention, there is provided one or more suitable pressure vessels made of stainless steel or other suitable material having the necessary strength andresistance to the corrosive action of fatty acids and water at high temperatures and pressures and of suflicient strengthto withstand the highrpressures used with an ample margin of safety. The arrangement of the apparatus is such that the fatty material and water or aqueous glycerine, which flow countercurrently, are in intimate contact over a relativel long path and do not have a tendency to emulsify to any great extent/ It is advantageous to cause the fatty material to flow upwardly through the vessel or vessels while the water or aqueous glycerine flows downwardly in intimate contact with it. Where a single pressure vessel is used, it may be provided on the inside with a number of trays or other suitable devices to insure intimate contact of the fatty material and the water or aqueous glycerine and to insure that this initimate contact is sufficiently prolonged to provide the desirable washing of glycerine from the fatty material which leads to the substantially complete hydrolysis of the present invention. Where a plurality of pressure vessels is used, the trays or other devices are not necessary, a the length of the path over' which the materials flow in contact is sufficient to accomplish the necessary intimacy and length of contact, but trays or similar devices may be provided with advantage if desired.

The apparatus is also provided with suitable heat exchangers, so that the heat contained in the outgoing fatty acids and glycerine solution may beused for the preheating of the water and fatty material fed to the apparatus, and with another heater or heaters between the heat exchangers and the apparatus to heat the fat or [5 fatty oil and water being supplied to the apparas as ault 7 -tu s to the necessary high temperature. Diphenyl heaters or high pressure steam heaters or other suitable heating means may be advantageously used for this purpose. 1 Suitable unitary heating units, such as electrical heaters properly placed around the exterior of the apparatus so that heat can be supplied to the apparatus where desired and in proper amounts to supply that lost by radiation and the like, are also advantageously provided. The apparatus is also provided with efficient insulation to minimize heat losses.

The apparatus is also suitably provided with pumps to introduce the water and fatt .oil or fat under the high pressure used, and with suitable gauges and thermometers and suitable safety devices such as safety valves and the like .to control the pressure and temperature within the apparatus.

It is advantageous to maintain the apparatus nearly full of the lighter fatty material and to maintain below the fatty material a settling zone for the separation of the aqueous solution from the fatty material. The apparatus is therefore provided with a suitable means of determining the position of the interface between the fatty material and the settling zone containing the quiescent aqueous glycerine near the point where the aqueous glycerine is removed, and near the point where the fat or fatty oil is introduced. The determination of the location of the oil or .fat and water interface may be accomplished by means of a gauge glass suitably located near the bottom of the apparatus, or by providing :a number of small faucets or outlets near the. bottom of the apparatus in vertical series.

The invention will be further illustrated by reference to the attached drawings-which illustrate an apparatus embodying the invention.

In the drawings,

Fig. 1 is a cross-sectional view of a pressure vessel which embodies the invention showing .an arrangement of trays within the vessel to provide a labyrinthal path for the material;

Fig. 2 is a cross-sectional view of a portion of a pressure vessel as in Fig. 1 showing a modified arrangement of trays within the vessel;

Fig 31 is an exterior view of a pressurevessel with the insulation removed showing the positioning of the electrical heaters used to provide suitable heating to onset losses by radiation;

Fig. 4 is an illustration of one type of *heat exchanger which may be used; and

Fig. 5 illustrates a diphenyl preheater which may be used.

One suitable construction of the interior of a pressure vessel is illustrated conventionally in Fig. l, the parts not being to scale. In thisfigure the vessel 22 may be, for example, two feet in diameter and fifteen feet high and may be made of suitable pressure-resistant and corrosionresistant material, such as stainless steel. It is shown as provided with a series of trays 23 and 23a, with the alternate trays 23a having a diameter the same as or somewhat less than :the

interior diameter of the vessel, andintermediate" trays 23 of smaller diameter, as shown. "These trays may be spaced, for example, about oneinch apart, more or less, but are shown as proportionately further apart, for convenience ofillustration. These trays are suitably supported by rods or other devices (not shown) and are ,so constructed and arranged as to cause the material passing through the vessel to, follow .labyrinthian ,-paths to increase the efliciency -of 8 the excess liquid water in washing glycerine from the fatty acids.

The alternate trays 23 are shown as of materially less diameter than the inner diameter of the vessel and as provided with rims at their outer peripheries over which the material flowing downwardly, that is, the aqueous glycerine or water, must flow; while the other trays 2301. which are shown as having the same diameter as the inner diameter of the vessel, but which may advantageously have a somewhat smaller diameter to allow for clearance and expansion, are also provided with outer peripheral rims and with openings at the center through which the water or glycerine must flow in its downward path. The fatty material, rising through the vessel, follows the reverse path.

At the bottom of the vessel is shown the settling zonefifi, in which the aqueous glycerine is separated from the fatty material. The aqueous glycerine, after proper separation, is removed through outlet 24, while the fatty material is fed to the apparatus through inlet 25 to a point advantageously above the lower trays and above the interface of the fatty material and the aqueous glycerine or water in the settling zone.

A somewhat similar zone 26 is provided at the top of the vessel for the separation of the fatty material from admixed water, so that the fatty material may be removed from the vessel free from any water except dissolved water. The fatty material, after proper separation, is removed through outlet 21 while water is introduced near the top of the vessel through inlet 28 to a point adjacent to the top tray of the vessel and below the separation zone. Faucets or outlets 35 may be advantageously provided near the bottom of the vessel to permit the determination of the position of the interface between the settling zone of aqueous glycerine and the fatty material. These faucets or outlets may be replaced or supplemented by a gauge glass of suitable strength and construction. Faucets or outlets 36 may also be provided at the middle and near the top of the vessel for drawing samples, and a safety valve 3! is also provided.

The vessel 22 is made of sufiicient strength to withstand the high pressures and temperatures used in the proces with an ample margin of safety and is advantageously made of a lower shell 29 and .an upper dome 39 advantageously provided with a suitable pressure-resistant gasket 32.

.In Fig. 2. is shown another modification of the trays which may be used within the pressure vessel of Fig. 1 to provide the necessary long path for the material to insure the .necessary intimacy of contact and completeness of reaction. In this modification, the holes in the trays 32 are made without rims,.alternate trays being provided with openings near the outer periphery while the other trays are provided with openings at the center; the water thus flowing downwardly in a labyrinthal path, while the fatty material flows upwardly following a reverse path. In Fig. 2, as in Fig. 1, the trays are shown spaced apart, for convenience of illustration, but may be, e. g., one inch apart in a vessel two feet in diameter. All of the holes in the trays, which may vary in location and arrangement, may have slight lips or -rims to retard the downward flow of the aqueous liquid.

Fig. 3 shows an arrangement by which the pressure vessel of Fig. 1 may be heated to counterbalance losses .due to radiation and the like. Thishgure shows how. on the exterior 0f the vessel, there may be provided a number of electrical heating units 33-, with electric connections 34, arranged in zones, so that heat supplied to various portions of the vessels, that is, the heat supplied for example to the upper portion and to the middle portions of the vessels may be varied independently, so that heat may be supplied locally to those portions of the apparatus where it is needed while avoiding an unnecessary input of heat and avoiding overheating those portions of the, apparatus where heat is not needed.

It is to be understood that suitable heat exchangers for the fatty material and water fed to the apparatus will be supplied, such heat exchangers as those shown in Fig. 4 being suitable, and that the material fed to the apparatus, after being preheated to use to advantage the heat contained in the fatty acids and aqueous glycerine taken from the apparatus, will be further heated by a suitable means, such as by a diphenyl heater as illustrated in Fig. 5. The apparatus will also be provided with efilcient insulation to conserve heat, and with suitable thermometers, such as thermocouples, located at various places throughout the apparatus to enable the temperatures of the material in the apparatus at various points to be determined and to enable the proper control of such temperatures. The apparatus will also be provided with suitable valves for controlling the input of water and fatty material, and for maintaining the pressure within the vessels at the proper point. Suitable pumps to force the water and fatty material in under the high pressures used will be provided.

The fatty material is introduced above the settling zone 20 by means of inlet 25, and the water is introduced below the settling zone 26 by means of inlet 28. The water and fatty material thus pass through the apparatus in countercurrent flow over a long path in intimate contact. The aqueous glycerine is removed from the bottom of the settling zone 20 by means of outlet 24, and the fatty acids are removed from the top of the settling zone 26 by means of outlet 21, the hot outgoing materials then passing. to suitable preheaters, such as shown in Fig. 4, where their contained heat is utilized for preheating fatty material and water fed to the apparatus.

1' have described the operation as a continuous process, with Water and fatty material continuously introduced into the apparatus in proper amounts, and proper proportions; and I prefer to operate the process in such continuous manner. Nevertheless, the process and apparatus may be operated in an intermittent or semi-continuous manner, with intermittent or alternate introduction of water and fatty material, within the scope of my invention in its broader aspects. Also, while I have described the invention as one involving the hydrolysis of fats and fatty oils by the use of liquid water alone, at high temperatures and pressures, it should be understood that if desired, and if unobjectionable, suitable catalysts may be used to speed up the hydrolysis.

The present application is a continuation of my prior application Serial No. 240,037, filed November 12, 1938, now abandoned, as a division of my application Serial No. 83,991, filed June 6, 1936, now Patent No. 2,139,589.

I claim:

1. Apparatus for the hydrolysis of fats and fatty oils comprising at least one pressure-resistant and corrosion-resistant elongated vertical 10 vessel, means for introducing fatty material near the bottom of said vessel, means for introducing aqueous liquid near the top of said vessel, a space for the separation of admixed and undissolved fatty material from aqueous glycerine near the bottom of said vessel and a space in saidvessel above the point of introduction of aqueous liquid for the separation of admixed and undissolved water from fatty material near the top of said vessel, means forremoval offatty material substantially free from admixed and undissolved water from fatty material, ,lheans for removal of aqueous glycerine free from admixed and undissolved fatty material from the bottom of said space provided near the bottom of said vessel for the separation of admixed and undissolved fatty material from aqueous glycerine, and a plurality of unitary heaters located along said vessel adapted to independently supply heat to various portions of the vessel whereby variations of temperatures within said various portions may be brought about or controlled.

2. The process for the hydrolysis of fats and fatty oils under pressure which comprises in troducing water near the top of an elongated vertical vessel and removing aqueous glycerine from the bottom thereof, introducing fatty material near the bottom of said vessel and removing fatty acids from the top thereof, the fatty material and water bein brought while under pressure and in liquid phases, into intimate contact in said vessel at a temperature of at least 200 C. at which the Water has appreciable solu- ,bility in the fatty material, separating admixed and undissolved water from the fatty acids at said pressure and above the point of introduction of the water and separating admixed and undisolved fatty material from the aqueous glycerine at said pressure.

3. The process for the hydrolysis of fats and fatty oils under pressure which comprises introducing water into the upper part of an elongated vessel and removing aqueous glycerine from a layer of aqueous glycerine in the lower part of said vessel, introducing fatty material above said layer of aqueous glycerine in the lower part of said vessel and removing fatty acids from a layer of fatty material in the upper part of said vessel, the fatty material and water being brought while under pressure and in liquid phases into intimate contact in said vessel at a temperature of at least 200 C. at which water has appreciable solubility in the fatty material, separating admixed and undissolved water from fatty acids in the upper part of said vessel while under pressure, and separating admixed and undissolved fatty material from said aqueous glycerine layer in the lower part of said vessel while under pressure.

4. In a countercurrent process of hydrolyzing fatty material with water, the steps comprising causing fatty material and Water to flow countercurrently in direct contact with each other through an elongated vertical vessel at a temperature above about 200 0.; introducing water and fat near the top and bottom of the column, respectively; withdrawing fatty acids and glycerine water from the top and bottom of the column, respectively; and supplying heat independently and locally to those portions of the vessel where it is needed while avoiding an unnecessary input of heat to those portions where heat is not needed.

MARTIN HILL ITTNER.

(References on following page) 2,009,510 Mobley July 30, 1935 '-.-2.'1:"'"'* '"-rrr M 1938 Haney Feb. 28, 1939 Mills May 2, 1939 June 27,1942; Murphy 4 V Feb. 26, 1943 R IGQ BA N' Country Date Great Bvitain June 2', 1932. Great-Bnitain V Sept. 29., 1932 

